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Lithium hydroxide, monohydrate → tert-butyl(E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valerate

HRID 1436138
ノート
印刷プレビュー

反応式

HRID 1436138 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[N:10]1[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]1)[CH:5]=O.[Cl:16][CH2:17][CH2:18][CH2:19][CH:20](P(OCC)(OCC)=O)[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22].O.[OH-].[Li+].O.C(=O)(O)[O-].[Na+]>C1COCC1.C(O)C>[Cl:16][CH2:17][CH2:18][CH2:19]/[C:20](=[CH:5]\[C:4]1[CH:7]=[CH:8][C:9]([N:10]2[CH:14]=[C:13]([CH3:15])[N:12]=[CH:11]2)=[C:2]([F:1])[CH:3]=1)/[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 168937Lithium hydroxide, monohydrateHCID 707008423-Fluoro-4-(4-methyl-1H-imidazol-1-yl)benzaldehydeHCID 86585896Sodium bicarbonate waterHCID 86602480Tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate

生成物 1

HCID 69004836tert-butyl(E)-5-chloro-2-{1-[3-fluoro-4-(4-methyl-1H-imidazol-1-yl)phenyl]methylidene}valerate収率 46.2%

試薬・触媒・溶媒

2
HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

3-Fluoro-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde (2.29 g) and tert-butyl 5-chloro-2-(diethoxyphosphoryl)valerate (3.68 g) were dissolved in a mixed solvent of THF (30 mL) and ethanol (10 mL). Lithium hydroxide monohydrate (1.41 g) was added to the reaction solution at room temperature, and the reaction solution was stirred at room temperature for 18 hours. Saturated sodium bicarbonate water was added to the reaction solution, followed by extraction with ethyl acetate. The resulting extract was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system), solidified with tert-butyl methyl ether and heptane, and separated by filtration to obtain 1.96 g of the title compound. The property values of the compound are as follows.

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. extractionThe resulting extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)
  6. customseparated by filtration

出典と根拠

ORDレコード
ord-e4245d1eb6c94ba9994356168e0a6688
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07618960B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート